WO1994017122A1 - Polyester material continuous crystallisation and polycondensation process - Google Patents
Polyester material continuous crystallisation and polycondensation process Download PDFInfo
- Publication number
- WO1994017122A1 WO1994017122A1 PCT/CH1994/000006 CH9400006W WO9417122A1 WO 1994017122 A1 WO1994017122 A1 WO 1994017122A1 CH 9400006 W CH9400006 W CH 9400006W WO 9417122 A1 WO9417122 A1 WO 9417122A1
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- WIPO (PCT)
- Prior art keywords
- polyester material
- temperature
- reactor
- polyester
- preheater
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/80—Solid-state polycondensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
- B29B13/065—Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/16—Auxiliary treatment of granules
- B29B2009/165—Crystallizing granules
Definitions
- the invention relates to a method for the continuous crystallization and polycondensation of polyester material according to the preamble of claim 1 and 2 respectively.
- the pre-crystallized material Before entering the reactor, the pre-crystallized material has to be heated to about 200 ° C. to 225 ° C. in the core and dried. The residence time in the reactor is again several hours. Surface temperatures of up to approx. 230 ° C are reached, which is already above the melting point, cf. z. B. EP-B-85 643. This in turn leads to signs of stickiness and agglomeration of the material in the thermal solid phase treatment.
- the invention is therefore based on the object, while avoiding the disadvantages of the prior art shown, of designing a process for the continuous crystallization and polycondensation of polyester material in such a way that exercises of the polyester material due to exothermic processes can be avoided.
- this object is achieved in that, in a process procedure known per se, as described, for.
- the material is subjected to intermediate cooling.
- the material is heated in the preheater from an initial temperature of, for example, 120-190 ° C. to approximately 220 ° C. in a hot gas stream and completely warmed up in a dwell time of approximately three hours.
- a degree of crystallinity of approx. 50% is achieved here.
- the residence time in the reactor is 7-15 hours in a known manner. A degree of crystallinity of about 53% is achieved. This is followed by conventional cooling of the material to ensure that it can be stored.
- the method according to the invention enables a higher application variance and an increased throughput of gas and polyester material. Material change and process change of an SSP system can be considerably simplified.
- the material throughput is used as a control variable to avoid the beginning of the melting of the polyester granulate.
- excess material is used, which results in a controlled temperature gradient. According to the invention, excess material is to be understood in the sense of a specific heat flow, derived from the required specific output
- CPG mean specific thermal conductivity.
- This variant of the invention is based on the surprising finding that an excess of gas tends to cause a deterioration in the temperature profile.
- a process control with transient driving is also possible.
- the material is preheated in a manner known per se in a few minutes in a gas stream of high temperature, but no total heating may occur. A degree of crystallinity of approx. 45% is achieved.
- the polyester material is heated in a fluidizing gas stream, for example air.
- the first fluidized bed is a bubbling fluidized bed with a mixed characteristic, in which the material has an average residence time of max. Is heated to about 160 ° C for 60 minutes.
- This is followed by a fluid bed as the second fluidized bed Piston flow characteristics, with heating to approx. 170 ° C, with a minimum residence time of 2-25 minutes. This ensures trouble-free and complete crystallization even of sticky material, and agglomerate-free granules with a uniform degree of crystallization are obtained.
- the polyester material is introduced into a preheater of an SSP reactor and in a period of about three hours to a temperature of about 215 ° C, max. 230 ° C heated with a hot inert gas stream (e.g. nitrogen). After passing through the preheating zone, the polyester material is intercooled from an average of 217 ° C. to approx. 210 ° C. in order to avoid overheating (exceeding the melting point) of the material in the subsequent reactor.
- a hot inert gas stream e.g. nitrogen
- the polyester material is again heated in the preheating zone of the reactor. In order to avoid the start of melting, however, an excess of material is used when a temperature of approximately 215 ° C. is reached.
- the material throughput is set in such a way that 218 ° C. is not exceeded and the granulate does not stick together.
- a temperature measurement is generally carried out in the process, and the data obtained can be compared with a simulation model.
Abstract
A process is disclosed for continuously crystallizing and polycondensating polyester material. The object of the invention is to avoid oxidative damages to the polyester material during the SSP treatment and at the same time to multiply the possibilities of application of polycondensation in the solid phase. For that purpose, the crystallized and polycondensed polyester material according to a per se known process is cooled by approximately 5 °C after going through the preheater and before entering the reactor.
Description
Beschreibung description
Verfahren zum kontinuierlichen Kristallisieren und Polykondensieren von PolyestermaterialProcess for the continuous crystallization and polycondensation of polyester material
Die Erfindung betrifft ein Verfahren zum kontinuierlichen Kristallisieren und Polykondensieren von Polyestermaterial nach dem Oberbegriff des Patentanspruchs 1 bzw. 2.2. The invention relates to a method for the continuous crystallization and polycondensation of polyester material according to the preamble of claim 1 and 2 respectively.
Es ist hinlänglich bekannt, Polyester-, bzw.Polyamidmaterial in zwei Verfahrensabschnitten kontinuierlich zu kristalli¬ sieren und nachfolgend in fester Phase zu polykondensieren. In einem stationären Betrieb erfolgt zunächst eine ein- und/oder zweistufige Kristallisation bei Temperaturen von 120 °C bis 190 °C und Verweilzeiten von bis zu mehreren Stunden. Zur Vermeidung von Verklebungen lehrt die EP-A-379 684 als besonders vorteilhafte .Anordnung die Führung des Materials durch hintereinander geschaltete Wirbelbetten. Das einen weitgehend einheitlichen Kristallinitätsgrad aufweisende Material wird anschliessend in einem Vorerhitzer erhitzt, ge¬ trocknet und teilweise polymerisiert, wobei die erforderliche Temperatur oberhalb der Oxidationstemperatur des Materials liegt. Von daher findet dieser Vorgang in einer Schutzgasat¬ mosphäre statt. Das vorkristallisierte Material muss vor dem Eintritt in den Reaktor auf ca. 200 °C bis 225 °C im Kern er¬ hitzt und getrocknet werden. Die Verweilzeit im Reaktor be¬ trägt wiederum mehrere Stunden. Hierbei werden Oberflächen¬ temperaturen bis ca. 230 °C erreicht, was bereits oberhalb des Schmelzpunktes liegt, vgl. z. B. EP-B-85 643. Dies wie¬ derum führt zu Klebrigkeitserscheinungen und Agglomeration des Materials bei der thermischen Festphasenbehandlung.It is well known to continuously crystallize polyester or polyamide material in two process stages and subsequently to polycondense in the solid phase. In a stationary operation, there is first a one and / or two-stage crystallization at temperatures from 120 ° C to 190 ° C and residence times of up to several hours. To avoid sticking, EP-A-379 684 teaches, as a particularly advantageous arrangement, the guidance of the material through fluidized beds connected in series. The material, which has a largely uniform degree of crystallinity, is subsequently heated, dried and partially polymerized in a preheater, the temperature required being above the oxidation temperature of the material. Therefore, this process takes place in a protective gas atmosphere. Before entering the reactor, the pre-crystallized material has to be heated to about 200 ° C. to 225 ° C. in the core and dried. The residence time in the reactor is again several hours. Surface temperatures of up to approx. 230 ° C are reached, which is already above the melting point, cf. z. B. EP-B-85 643. This in turn leads to signs of stickiness and agglomeration of the material in the thermal solid phase treatment.
Der Erfindung liegt daher die Aufgabe zugrunde, unter Vermei¬ dung der aufgezeigten Nachteile des Standes der Technik ein Verfahren zum kontinuierlichen Kristallisieren und Polykon¬ densieren von Polyestermaterial so auszubilden, dass Verkle-
bungen des Polyestermaterials infolge exothermer Abläufe vermieden werden.The invention is therefore based on the object, while avoiding the disadvantages of the prior art shown, of designing a process for the continuous crystallization and polycondensation of polyester material in such a way that exercises of the polyester material due to exothermic processes can be avoided.
Diese Aufgabe wird erfindungsgemäss dadurch gelöst, dass in einer an sich bekannten Verfahrensführung, wie sie z. B. in der EP-A-379 684 offenbart wird, nach dem Austritt des Mate¬ rials aus dem Vorerhitzer und vor dem Eintritt in den Reaktor das Material einer Zwischenkühlung unterworfen wird. Bei einer solchen Verfahrensführung mit stationärem Gleichgewicht wird das Material im Vorerhitzer von einer Ausgangstemperatur von beispielsweise 120-190 °C auf ca. 220 °C im heissen Gas¬ strom erhitzt und in einer ca. dreistündigen Verweildauer vollständig durchgewärmt. Hierbei wird ein Kristallinitäts- grad von ca. 50 % erreicht. Beim Übertritt des Materials in den Reaktor und weiterer Durchströmung mit heissem Gas führen bei der bekannten Verfahrensführung exotherme Vorgänge im dichtgepackten Materialstrom zu Verklebungen des Materials.According to the invention, this object is achieved in that, in a process procedure known per se, as described, for. As is disclosed in EP-A-379 684, after the material has left the preheater and before entering the reactor, the material is subjected to intermediate cooling. In such a process with steady-state equilibrium, the material is heated in the preheater from an initial temperature of, for example, 120-190 ° C. to approximately 220 ° C. in a hot gas stream and completely warmed up in a dwell time of approximately three hours. A degree of crystallinity of approx. 50% is achieved here. When the material passes into the reactor and hot gas flows through it further, exothermic processes in the densely packed material flow lead to sticking of the material in the known process.
Es wurde nun gefunden, dass diese Nachteile durch eine Zwi¬ schenkühlung des Materials vermeidbar sind. Die Abkühlung er¬ folgt, in Abhängigkeit vom verwendeten Polyestermaterial um ca. 5 °C gegenüber der erreichten Endtemperatur im Vorerhit¬ zer, um ein Erreichen oder gar Überschreiten einer kritschen Oberflächentemperatur (Beginn des Aufschmelzens) zu verhin¬ dern.It has now been found that these disadvantages can be avoided by intercooling the material. The cooling takes place, depending on the polyester material used, by approx. 5 ° C. compared to the final temperature reached in the preheater in order to prevent a critical surface temperature from being reached or even exceeded (beginning of melting).
Die Verweilzeit im Reaktor beträgt in bekannter Weise 7-15 Stunden. Erreicht wird ein Kristallinitätsgrad von etwa 53 %. Anschliessend folgt eine übliche Kühlung des Materials, um die Lagerfähigkeit zu gewährleisten.The residence time in the reactor is 7-15 hours in a known manner. A degree of crystallinity of about 53% is achieved. This is followed by conventional cooling of the material to ensure that it can be stored.
Eine solch einfache Verfahrensweise war aus dem Stand der Technik nicht folgerbar, wurde doch vielmehr eine einge¬ schränkte Verfahrensweise und eine mögliche, oxidative Schä¬ digung bewusst in Kauf genommen (DE-AS 25 58 730,
DE-OS 26 42 102) oder es wurden zusätzliche Verfahrensschrit¬ te und Substanzen vorgeschlagen (z. B. US-PS 4 130 551, DE-OS 21 24 203) .Such a simple procedure could not be inferred from the prior art, but rather a restricted procedure and possible oxidative damage were consciously accepted (DE-AS 25 58 730, DE-OS 26 42 102) or additional method steps and substances have been proposed (e.g. US Pat. No. 4,130,551, DE-OS 21 24 203).
Des weiteren ermöglicht die erfindungsgemässe Verfahrens¬ führung eine höhere Anwendungsvarianz und einen erhöhten Durchsatz an Gas und Polyestermaterial. Materialwechsel und Prozessänderung einer SSP-Anlage können wesentlich verein¬ facht werden.Furthermore, the method according to the invention enables a higher application variance and an increased throughput of gas and polyester material. Material change and process change of an SSP system can be considerably simplified.
In einer Ausgestaltung der Erfindung wird anstelle einer Zwi¬ schenkühlung im Gasstrom der Materialdurchsatz als Regel- grösse zur Vermeidung des Aufschmelzbeginns des Polyestergra¬ nulats verwendet. Dabei wird nach dem Vorerhitzen im Reaktor mit Materialüberschuss gefahren, was einen kontrollierten Temperaturgradienten ergibt. Materialüberschuss ist erfin- dungsgemäss im Sinne eines spezifischen Wärmestroms zu ver¬ stehen, abgeleitet von der notwendigen spezifischen Leistung gemässIn one embodiment of the invention, instead of intermediate cooling in the gas stream, the material throughput is used as a control variable to avoid the beginning of the melting of the polyester granulate. After preheating in the reactor, excess material is used, which results in a controlled temperature gradient. According to the invention, excess material is to be understood in the sense of a specific heat flow, derived from the required specific output
ms • cps > ig . cpg wobei m s • cp s > ig. cpg where
ms Massestrom Granulat cPs spezifische Wärmeleitfähigkeit Granulat mg Massestrom Gasm s mass flow granulate cPs specific thermal conductivity granulate mg mass flow gas
CPG spezifische Wärmeleitfähigkeit bedeuten.CPG mean specific thermal conductivity.
Dieser Variante der Erfindung liegt die überraschende Er¬ kenntnis zugrunde, dass ein Gasüberschuss eher eine Ver¬ schlechterung des Temperaturprofils bewirkt.This variant of the invention is based on the surprising finding that an excess of gas tends to cause a deterioration in the temperature profile.
II.
Eine solche Lösung ist dem bekannten Stand der Technik nicht zu entnehmen. Sie liegt die DE-AS 25 29 290 ein Gewichtsver¬ hältnis Gasstrom (Stickstoff) zu Granulat von 2 : 1 zugrunde,
d.h. ein deutlicher Gasüberschuss. Gemäss EP-B-310 968 kann bei einer Kristallisation anhand der Materialtemperatur die Entnahmegeschwindigkeit des Granulats geregelt werden. Daraus ist jedoch nicht ableitbar, wie mit dem Massestrom selbst ein Beginn des Anschmelzens vermieden werden kann.Such a solution cannot be found in the known prior art. It is based on DE-AS 25 29 290, a weight ratio of gas stream (nitrogen) to granules of 2: 1, ie a significant excess of gas. According to EP-B-310 968, the rate of removal of the granules can be regulated in the case of crystallization on the basis of the material temperature. However, it cannot be deduced from this how the start of the melting process can be avoided with the mass flow itself.
In der nicht vorveröffentlichten schweizerischen Patentanmel¬ dung Nr. 02 516/92-0 der Anmelderin wird ebenso vermekrt, dass Regelungen über die Temperatur relativ träge sind und eine Regelung über die Verweilzeit des Materials im Reaktor und/oder der Vorheizzone möglich ist. D.h. Beeinflussung durch die auszutragende Materialmenge pro Zeiteinheit.In the applicant's previously unpublished Swiss patent application No. 02 516 / 92-0, it is also noted that regulations about the temperature are relatively slow and regulation about the residence time of the material in the reactor and / or the preheating zone is possible. That Influenced by the amount of material to be discharged per unit of time.
Neben dem vorgenannten ist in einer anderen Ausgestaltung der Erfindung auch eine Verfahrensführung mit instationärer Fahr¬ weise möglich. Hierzu erfolgt die Vorerhitzung des Materials in an sich bekannter Weise in wenigen Minuten in einem Gas¬ strom von hoher Temperatur, wobei jedoch keine totale Durch¬ wärmung eintreten darf. Erreicht wird ein Kristallinitatsgrad von ca. 45 %.In addition to the above, in another embodiment of the invention, a process control with transient driving is also possible. For this purpose, the material is preheated in a manner known per se in a few minutes in a gas stream of high temperature, but no total heating may occur. A degree of crystallinity of approx. 45% is achieved.
Die weiterführende Behandlung im Reaktor mit nachfolgender Kühlung lässt wiederum einen Kristallinitatsgrad von ca. 53 % erreichen, jedoch bei höherer Exothermie.Further treatment in the reactor with subsequent cooling in turn allows a degree of crystallinity of approx. 53% to be achieved, but with higher exothermicity.
Das erfindungsgemässe Verfahren soll nachstehend an Hand eines Ausführungsbeispieles näher beschrieben werden.The method according to the invention will be described in more detail below using an exemplary embodiment.
Beispiel 1example 1
In einer Anordnung gemäss EP-A-379 684, bestehend aus zwei hintereinander geschalteten Wirbelbetten, wird das Polyester¬ material in einem Fluidisiergasstrom, beispielsweise Luft, erhitzt. Das erste Wirbelbett ist ein sprudelndes Wirbelbett mit Mischcharakteristik, in dem das Material bei einer mitt¬ leren Verweildauer von max. 60 Minuten auf ca. 160 °C erwärmt wird. Dem folgt als zweites Wirbelbett ein Fliessbett mit
Kolbenströmungscharakteristik, mit einer Erwärmung auf ca. 170 °C, bei einer Mindestverweildauer von 2-25 Minuten. Damit ist eine störungsfreie und vollständige Kristallisation selbst von klebrigem Material gewährleistet, es wird ein agglomeratfreies Granulat von einheitlichem Kristallisa¬ tionsgrad erhalten.In an arrangement according to EP-A-379 684, consisting of two fluidized beds connected in series, the polyester material is heated in a fluidizing gas stream, for example air. The first fluidized bed is a bubbling fluidized bed with a mixed characteristic, in which the material has an average residence time of max. Is heated to about 160 ° C for 60 minutes. This is followed by a fluid bed as the second fluidized bed Piston flow characteristics, with heating to approx. 170 ° C, with a minimum residence time of 2-25 minutes. This ensures trouble-free and complete crystallization even of sticky material, and agglomerate-free granules with a uniform degree of crystallization are obtained.
Nach dem Kristallisationsvorgang wird das Polyestermaterial in einen Vorerhitzer eines SSP-Reaktors eingebracht und in einem Zeitraum von ca. drei Stunden auf eine Temperatur von ca. 215 °C, max. 230 °C mittels eines heissen Inertgasstroms (z.B. Stickstoff) erhitzt. Nach dem Passieren der Vorheizzone wird das Polyestermaterial von durchschnittlich erreichten 217 °C auf ca. 210 °C zwischengekühlt, um eine Überhitzung (Überschreitung des Schmelzpunktes) des Materials im nachfol¬ genden Reaktor zu vermeiden.After the crystallization process, the polyester material is introduced into a preheater of an SSP reactor and in a period of about three hours to a temperature of about 215 ° C, max. 230 ° C heated with a hot inert gas stream (e.g. nitrogen). After passing through the preheating zone, the polyester material is intercooled from an average of 217 ° C. to approx. 210 ° C. in order to avoid overheating (exceeding the melting point) of the material in the subsequent reactor.
Im Reaktor, beschrieben z. B. in der EP-A-379 684, erfolgt eine Nachkondensation des Materials in fester Phase bei einer Temperatur von weniger als 217 °C und einer Verweildauer von 7-10 Stunden. Nachfolgend wird das fertige Granulat auf eine Temperatur von weniger als 60 °C gekühlt, um dessen Lagerfä¬ higkeit zu sichern.In the reactor, described for. B. in EP-A-379 684, there is a post-condensation of the material in the solid phase at a temperature of less than 217 ° C and a residence time of 7-10 hours. The finished granulate is then cooled to a temperature of less than 60 ° C. in order to ensure its storability.
Beispiel 2Example 2
Nach einer Kristallisation gemäss Beispiel 1 erfolgt wiederum eine Erhitzung des Polyestermaterials in der Vorheizzone des Reaktors. Zur Vermeidung des Anschmelzbeginns wird jedoch bei Erreichen einer Temperatur von ca. 215°C mit einem Material¬ überschuss gefahren. Der Materialdurchsatz wird so einge¬ stellt, dass 218°C nicht überschritten werden und ein Verkle¬ ben des Granulats unterbleibt.After crystallization according to Example 1, the polyester material is again heated in the preheating zone of the reactor. In order to avoid the start of melting, however, an excess of material is used when a temperature of approximately 215 ° C. is reached. The material throughput is set in such a way that 218 ° C. is not exceeded and the granulate does not stick together.
Generell erfolgt eine Temperaturmessung im Prozess, ein Ver¬ gleich der gewonnenen Daten mit einem Simulationsmodell, ist möglich.
A temperature measurement is generally carried out in the process, and the data obtained can be compared with a simulation model.
Claims
1. Verfahren zum kontinuierlichen Kristallisieren und Fest- phasen-Polykondensieren von Polyestermaterial durch Kri¬ stallisieren des Ausgangsmaterials, nachfolgender Vor¬ heizung des vorkristallisierten Materials und Polykon¬ densation bei ca. 205 °C bis 230 °C in fester Phase sowie anschliessender Abkühlung, dadurch gekennzeichnet, dass das Polyestermaterial nach dem Passieren des Vorerhitzers, vor dem Eintritt in den Reaktor einer Zwischenkühlung aus¬ gesetzt wird.1. A process for the continuous crystallization and solid-phase polycondensation of polyester material by crystallizing the starting material, subsequent preheating of the precrystallized material and polycondensation at about 205 ° C. to 230 ° C. in the solid phase and subsequent cooling, thereby characterized in that the polyester material after passing through the preheater is subjected to intermediate cooling before entering the reactor.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Zwischenkühlung in Abhängigkeit vom Polyestermaterial auf eine Temperatur unterhalb einer kritischen Oberflä¬ chentemperatur (Aufschmelzbeginn) des Polyestermaterials erfolgt.2. The method according to claim 1, characterized in that the intermediate cooling takes place depending on the polyester material to a temperature below a critical surface temperature (start of melting) of the polyester material.
3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, dass das Polyestermaterial gegenüber der Vorerhitzertempe¬ ratur vorzugsweise um mindestens 5 °C abgekühlt wird.3. The method according to claim 1 and 2, characterized in that the polyester material compared to the preheater temperature is preferably cooled by at least 5 ° C.
4. Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, dass das Vorerhitzen des Polyestermaterials durch eine in¬ stationäre Kurzzeitvorerhitzung von nur wenigen Minuten Dauer und bei einer genügend hohen Temperatur erfolgt. 4. The method according to claim 1 to 3, characterized in that the preheating of the polyester material is carried out by in¬ stationary short-term preheating of only a few minutes and at a sufficiently high temperature.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH179/93-5 | 1993-01-21 | ||
CH17993A CH684697A5 (en) | 1993-01-21 | 1993-01-21 | A method of continuously crystallizing and polycondensing polyester material. |
Publications (1)
Publication Number | Publication Date |
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WO1994017122A1 true WO1994017122A1 (en) | 1994-08-04 |
Family
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Family Applications (1)
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PCT/CH1994/000006 WO1994017122A1 (en) | 1993-01-21 | 1994-01-11 | Polyester material continuous crystallisation and polycondensation process |
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CH (1) | CH684697A5 (en) |
WO (1) | WO1994017122A1 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19505680C1 (en) * | 1995-02-20 | 1996-05-23 | Inventa Ag | Condensn. injection moulding of preform for food-quality bottle |
WO2007022994A1 (en) | 2005-08-26 | 2007-03-01 | Lurgi Zimmer Gmbh | Method and device for reducing acetaldehyde content in polyester granulate |
US7262263B2 (en) | 2001-11-30 | 2007-08-28 | Brigitta Otto | Method and apparatus for producing solid-state polycondensed polyesters |
US7977448B2 (en) | 2004-03-04 | 2011-07-12 | Lurgi Zimmer Gmbh | Method for producing highly condensed solid-phase polyesters |
US8063176B2 (en) | 2006-03-16 | 2011-11-22 | Lurgi Zimmer Gmbh | Method and device for the crystallization of polyester material |
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FR2008523A1 (en) * | 1968-05-14 | 1970-01-23 | Glanzstoff Ag | |
US4161578A (en) * | 1978-05-12 | 1979-07-17 | Bepex Corporation | Process for solid phase polymerization of polyester |
EP0085643A2 (en) * | 1982-02-02 | 1983-08-10 | The Goodyear Tire & Rubber Company | Process for the production of high molecular weight polyester |
EP0091566A1 (en) * | 1982-04-02 | 1983-10-19 | Karl Fischer Industrieanlagen Gmbh | Process and apparatus for the post condensation of polycondensates |
EP0379684A2 (en) * | 1988-12-23 | 1990-08-01 | Bühler Ag | Method of and apparatus for the continuous crystallisation of polyesters |
-
1993
- 1993-01-21 CH CH17993A patent/CH684697A5/en not_active IP Right Cessation
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1994
- 1994-01-11 WO PCT/CH1994/000006 patent/WO1994017122A1/en active Application Filing
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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FR2008523A1 (en) * | 1968-05-14 | 1970-01-23 | Glanzstoff Ag | |
US4161578A (en) * | 1978-05-12 | 1979-07-17 | Bepex Corporation | Process for solid phase polymerization of polyester |
EP0085643A2 (en) * | 1982-02-02 | 1983-08-10 | The Goodyear Tire & Rubber Company | Process for the production of high molecular weight polyester |
EP0091566A1 (en) * | 1982-04-02 | 1983-10-19 | Karl Fischer Industrieanlagen Gmbh | Process and apparatus for the post condensation of polycondensates |
EP0379684A2 (en) * | 1988-12-23 | 1990-08-01 | Bühler Ag | Method of and apparatus for the continuous crystallisation of polyesters |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19505680C1 (en) * | 1995-02-20 | 1996-05-23 | Inventa Ag | Condensn. injection moulding of preform for food-quality bottle |
US5656719A (en) * | 1995-02-20 | 1997-08-12 | Ems-Inventa Ag | Condensation injection molding process for producing bottle preforms of polyethylene terephthalate and/or its copolyesters and resultant preforms |
US7262263B2 (en) | 2001-11-30 | 2007-08-28 | Brigitta Otto | Method and apparatus for producing solid-state polycondensed polyesters |
US7977448B2 (en) | 2004-03-04 | 2011-07-12 | Lurgi Zimmer Gmbh | Method for producing highly condensed solid-phase polyesters |
WO2007022994A1 (en) | 2005-08-26 | 2007-03-01 | Lurgi Zimmer Gmbh | Method and device for reducing acetaldehyde content in polyester granulate |
US7521522B2 (en) | 2005-08-26 | 2009-04-21 | Lurgi Zimmer Gmbh | Method and device to reduce the acetaldehyde content of polyester granulate |
US8063176B2 (en) | 2006-03-16 | 2011-11-22 | Lurgi Zimmer Gmbh | Method and device for the crystallization of polyester material |
Also Published As
Publication number | Publication date |
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CH684697A5 (en) | 1994-11-30 |
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